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On the Role of Turbostratic Graphite in the Crystallization of Spheroidal

Graphite During the Liquid-to-Solid Transformation

Article in Metallurgical and Materials Transactions B · July 2023

DOI: 10.1007/s11663-023-02854-w

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 BRIEF COMMUNICATION

On the Role of Turbostratic Graphite

in the Crystallization of Spheroidal Graphite During
the Liquid-to-Solid Transformation
DORU MICHAEL STEFANESCU, TOMASZ TOKARSKI, GORKA ALONSO,
MARCIN GÓRNY, and RAMÓN SUÁREZ

While turbostratic graphite is documented in many forms of graphite, there is a paucity of

information on its contribution to the crystallization of spheroidal graphite (SG) in cast iron.
SAD on SG and discussion of deep-etched SEM samples, demonstrates that it is an integral part
of the crystallization sequence of SG. It is found in the core region, but also in the outer shell.
This imposes a reevaluation of current theories of SG crystallization.

https://doi.org/10.1007/s11663-023-02854-w
 The Minerals, Metals & Materials Society and ASM International 2023

CARBON can form various allotropes ranging from
amorphous structure to fully crystalline hexagonal
graphite. Turbostratic structure is one of the possible
forms of graphite characterized by specific disordering
of graphene layers. Contrary to the crystalline hexago-
nal graphite, there is no ordering between consecutive
graphene layers, i.e., each layer can be randomly rotated
around the c-axis (perpendicular to graphene layer).
Additionally, turbostratic graphite can have various
levels of disordering, including rotation, translation, and
curvature of layers.[1,2] Thus, turbostratic graphite could
be considered a special case of highly defected crystalline
graphite. With a one-dimensional periodicity only,
turbostratic graphite is neither crystalline nor amor-
phous. This defect produces the specific elliptic-like
shape in Transmission Electron Microscopy (TEM)
diffraction patterns, a phenomenon accurately described
by Rouzaud and Oberlin.[3]
After the invention of ductile iron in 1943, the
crystallization of spheroidal graphite (SG) from the
melt has been extensively studied and covered in many
review papers, such as the one by Merchant[4] that goes
back to the early paper of Morrogh and Williams,[5] and
the more recent ones (e.g.,[6]) that describes the current
DORU MICHAEL STEFANESCU is with the The University of
Alabama, Tuscaloosa, AL 35487 and also with the Ohio State
University, Columbus, OH 43210. Contact e-mail:
stefanescu.1@osu.edu TOMASZ TOKARSKI and MARCIN
GÓRNY are with the AGH University of Science and Technology,
30-059 Kraków, Poland. GORKA ALONSO and RAMÓN SUÁREZ
are with the Azterlan, Basque Research and Technology Alliance
(BRTA), 48200 Durango, Spain.
Manuscript submitted March 11, 2023; accepted June 19, 2023.
Article published online July 21, 2023.
understanding of SG crystallization in cast iron. New
research[7] demonstrates that turbostratic graphite
appears to be part of the crystallization process of
carbon during graphite growth on its nucleus. However,
research establishing the presence of this type of
graphite in cast iron has been minimal, while informa-
tion and discussion of the role of turbostratic graphite in
the growth of spheroidal graphite is all but inexistent.
This is a knowledge gap that this communication
attempts to fill, by demonstrating the presence of
turbostratic graphite across various sections of the
graphite spheroid.
Analysis of the graphitization of pyrolyzed anthra-
cene heat treated up to 2900 C by Rouzaud and
Oberlin[3] provides excellent background for under-
standing the crystallization of graphite in carbonaceous
materials. Based on TEM data, the graphitization
process was divided into four stages. In the first stage,
basic structural units (SU) thinner than l nm and of
length ~ 1 to 2 nm, aggregate in relatively parallel areas
separated by tilt/twist boundaries and other defects
(Figure 1(a)). In stage 2, structural units (SU) aggregate
face to face into distorted columns. Lateral growth is
inhibited by misoriented single SU. In stage 2, disorga-
nized, thin columns evolve (Figure 1(b)). In stage 3,
graphite layers stack into distorted columns (Fig-
ure 1(c)). As the annealing temperature increases from
1600 C to 1800 C the columns coalesce into parallel
wrinkled layers. According to Rouzaud and Oberlin,
graphitization occurs from the beginning of stage 4.
However, the images in stage 3 appear to show some
turbostratic graphite, as it will be demonstrated later in
this paper, and growth of turbostratic graphite is part of
the graphitization process. During stage 4 most defects
are eliminated, and the distortions are annealed (Fig-
ure 1(d)). Selected area electron diffraction (SAD)

METALLURGICAL AND MATERIALS TRANSACTIONS B VOLUME 54B, OCTOBER 2023—2283

Fig. 1—Dark field images of graphite during graphitization stages: (a) stage 1; (b) stage 2; (c) stage 3; (d) stage 4. Reprinted with permission
from Ref. [3].
revealed turbostratic graphite in stage 2 and 3. Graphi-
tization occurs after development of two-dimensional
order by de-wrinkling of the turbostratic structure. The
schematic representation of stage 3 by Rouzaud and
Oberlin resembles what is later referred to as ‘‘herring-
bone’’ structure in spheroidal graphite (SG).
Graphite spheroids are one of the most intriguing
forms of aggregation of graphite, by no means specific
only to cast iron, as they can be found as natural formed
graphite in meteorites or in metamorphic graphite, as
well as in many man-made products. SG cast iron is one
of the most important materials used in contemporary
engineering. Recent work on turbostratic graphite in
iron imposes a reevaluation of current theories of SG
crystallization.
There are two main theories on the growth of
spheroidal graphite: (i) one-stage growth of cylindrical
columns or of conical sectors, similar to the pyramidal
sectors found in ice and silicon crystals; (ii) multi-stage
growth including growth of curved platelets in contact
with the liquid (stage I), followed by growth of columns
and/or conical sectors through the solid austenite shell
during the eutectic reaction (stage II), and then growth
during the solid-solid transformation (stage III) illus-
trated through optical and SEM microscopy in Figure 2.
2284—VOLUME 54B, OCTOBER 2023
Proponents of the one-stage theory offer several
possible mechanisms. The cone-helix (micro-spiral)
growth mechanism of Double and Hellawell[8] assumes
growth in the c-direction through spiral growth (Fig-
ure 3(a)). This model may explain the herringbone
appearance of graphite platelets in some spheroids
(Figure 2(c)) and is also consistent with the observation
that the growing ends of whiskers produced through
carbon pyrolysis assumed a conical shape.[9] Miao
et al.[10] suggested that the spiral-dislocation growth of
conical sectors, composed of rhombohedral graphite
platelets, occurs in a direction nearly parallel to the
<001> direction of graphite (Figures 3(b) and (c)).
Based on their Figure 2 it is estimated that the platelets
are 40 to 60 nm thick and lm long. Platelets 20 nm thick
were also identified in spheroidal graphite nodules in
steel.[11] Another possible mechanism for the formation
of columns is poly-nucleation (PNG). It assumes that
many 2-D nuclei form on the surface of a growing
graphite platelets.[1] An example of such nucleation on
spherical metamorphic graphite is shown in Figure 7 in
Reference 12. Growth of conical sectors made of
hexagonal graphite platelets parallel to one another
appears to be the dominant mechanism in spheroidal
graphite formed in annealed medium-carbon steel[13]
METALLURGICAL AND MATERIALS TRANSACTIONS B
Fig. 2—Growth stages of SG in Fe–C–Si alloys: (a) optical image of SG (compliments of J. Barlow and A. Catalina, Caterpillar Inc.); (b) and
(c) SEM images of chemically etched SG on specimens quenched during solidification; (d) SEM plasma etched SG with a MgS nucleus (Courtesy
of J.R. Hitchings, Comanche Technologies).

Fig. 3—Growth mechanisms of conical sectors: (a) cone-helix model; reprinted with permission from Ref. [8]; (b) spiral-dislocation model;
reprinted with permission from Ref. [10]; (c) structure of a cone produced through spiral-dislocation growth; reprinted with permission from Ref.
[10].

METALLURGICAL AND MATERIALS TRANSACTIONS B VOLUME 54B, OCTOBER 2023—2285

and in pyrolytic graphite spheres.[1] It was also identified
in SG formed in cast iron (e.g., References 14–16).
However, the graphite spheroids in Figure 2 show a
clear distinction between graphite solidified during stage
I and graphite growing during stage II. A striking
example of 2-stage growth is shown in Figure 4 where
curved concentric graphite layers are seen in stage I,
confirming the concentric platelets in Figure 2. Columns
that entrap iron in between are characteristic for stage
II. There is no iron entrapment in the first stage. The
inset shows columnar growth originating on the
graphite platelets formed in stage I. These, and many
other similar images have led other researchers (e.g.,
References 17–19) to support the multi-stage theory.
For stage I Sadocha and Gruzlesky[20] postulated SG
crystallization through curved circumferential growth of
hexagonal graphite layers. Direct SEM observation of
deep-etched SG growing out of Ni-3 pct C melts in
Figure 5, indisputably shows both the 2-stage growth
with curved graphite platelets in stage I and columns in
stage II.[17]
High-resolution 3D tomography by Ghassemali
et al.[21] further supports a curved-circumferential
growth mechanism in stage I, as concentrically dis-
tributed pores formed during this stage I (Figures 6(a)
and (c)). In stage II channel-like iron inclusions are
distributed radially throughout the graphite outlining
conical sectors (Figures 6(a) and (b)). They do not
penetrate the core.
Regarding stage III, Purdy and Audier[22] postulate
that carbon is transported by diffusion through the
austenite shell and is deposited at the iron/graphite
interface as amorphous carbon that crystallizes upon
cooling. Such amorphous carbon layers have also been
identified by Qing et al.[18]
Fig. 4—SEM plasma etched graphite spheroid showing 2-stage growth. Courtesy of J.R. Hitchings, Comanche Technologies.
2286—VOLUME 54B, OCTOBER 2023
Yet, the theory of nicely ordered curved graphite
platelets surrounding the nucleus is challenged by recent
research. TEM analysis of graphite extracted from SG
iron by Hara et al.[14] concluded that SG had a
three-stage internal structure with annular rings of a
layered intermediate region, and an outer region of large
polygonal crystalline plates (Figure 7(a)). However, the
central region exhibited bent graphene layers (Fig-
ure 7(b)) or, according to the authors, had an amor-
phous-like appearance (Figure 7(c)). Furthermore,
interrupted solidification experiments appear to show a
different picture for the stage I.[23] While curved platelets
appear to grow around the nucleus, a closer look
reveals, in some instances, rather distorted short
platelets separated by voids, as in Figure 2(b),[26] and
even herringbone platelets as in Figure 2(c) and in
Reference 24. We notice that, while according to Hara
et al. the image in Figure 7(b) exhibits ‘‘bent graphene
layers’’, the elliptic diffraction pattern suggests tur-
bostratic graphite, a structure not mentioned in the
paper.
High-resolution TEM (HRTEM) images for carbon
spheroids in cast iron and steel tell a similar story.
Indeed, Qing et al.[25] show that for SG in cast iron,
images of the graphite lattice near the nucleus exhibit
high curvature and high density of crystallographic
defects. Moreover, an SAD pattern obtained in a sub
grain formed during stage 2 showed a single c-axis
direction, in contrast to the multiple c-axis directions on
an SAD pattern from the center of graphite particle, i.e.,
all graphite nodules begin with identical structures of
spherically curved basal planes. Images from areas of a
nodule from heat treated steel examined by He et al.[13]
show a regular arrangement of the graphite (002) planes
(graphene layers) in areas near the edge of the spheroid,
METALLURGICAL AND MATERIALS TRANSACTIONS B
Fig. 5—SEM of graphite aggregates in a Ni-3 pct C alloy: (a) spheroid showing curved growth of graphite platelets; (b) spheroid showing stage
II growth of columnar graphite; reprinted with permission from Ref. [17].

Fig. 6—High-resolution 3D tomography of a graphite spheroid: (a) 2D distribution of voids and Fe channels; (b) Fe distribution in a thin disk
cut at the center of the graphite spheroid; (c) 2D distribution of voids; reprinted with permission from Ref. [21].

Fig. 7—TEM bright field image of spheroidal graphite (a) and SAD patterns and inverse Fast Fourier Transform (FFT) processed images
obtained for points  and ` (b) and (c); adapted after Ref. [14].

METALLURGICAL AND MATERIALS TRANSACTIONS B VOLUME 54B, OCTOBER 2023—2287

but ‘‘near-amorphous’’ appearance in the proximity of
the center.
In schematic synopsis of multi-stage mechanisms by
various investigators[17–19] the curved platelets are cir-
cumferential and concentric but do not grow in a
continuous spiral as in the Sadocha/Gruzlesky model.
For a more detailed discussion of these and other
models the reader is directed to the recent review in
Reference 26.
Thus, in some instances stage I growth produces an
ordered layer, while in other instances the microstruc-
ture in the vicinity of the nucleus exhibits disordered and
bent platelets as in Figures 2(b) and (c), or even
‘‘amorphous’’ graphite like in Figure 7. What is the
reason for the variety of structures seen in stage I
growth? The growth of a graphite spheroid out of liquid
iron includes crystallization of carbon that starts imme-
diately after its nucleation and continues to room
temperature. This is also typical for annealed steel and
was also demonstrated by heating amorphous carbon in
an electronic beam.[27] Early graphite structure may
have a low degree of crystallinity, consistent with
observations on quenched specimens. Room-tempera-
ture graphite may be fully crystallized but still exhibits
many defects.
The presence of turbostratic graphite was previously
discussed by Pencea et al.[28] using wide-angle X-ray
diffraction, and by Ohbuchi et al.[29] using X-ray powder
diffractometry. The latter paper disclosed that 32 pct of
the total mass of graphite in the SG iron under
investigation was turbostratic graphite, while 68 pct
was crystalline graphite. However, the experimental
method did not allow for a detailed analysis of the
location of the turbostratic graphite within the graphite
spheroid.
Recently, Alonso et al.[7] addressed the graphite
structure in the immediate neighborhood of the gra-
phite/nucleus in a SG iron specimen. Turbostratic
graphite was identified at the interface. Figure 8 presents
SAED images at the (Mg,Si,Al)N nitride
Fig. 8—SAED patterns at a (Mg,Si,Al)N nitride/graphite interface. Numbered circles indicate the position of the diffraction aperture moved
sequentially away from the nitride interface (1) to the graphite region (4); reprinted with permission from Ref. [7].
2288—VOLUME 54B, OCTOBER 2023
nucleus/graphite interface. The nitride signal dominates
the first two diffraction images (1) and (2). Blurred,
ellipsoidal effects corresponding to Debye–Scherrer
rings of turbostratic graphite are seen on all images.
Diffraction spots from graphite appear in image (4). It
can thus be concluded that a layer of turbostratic
graphite, at least 0.1 lm thick, grows on the surface of
the nucleus. Debye–Scherrer pattern with hk ellipses was
also identified by Bourdie et al.[16] in the proximity of
the SG core but was attributed to mechanical straining
associated with solidification.
SAED patterns obtained at various distance from the
nucleus confirm that a crystalline region can grow in the
immediate proximity of the nucleus (Figure 9(a)), while
turbostratic regions are found both in the vicinity of the
nucleus (Figure 9(b)) that is in stage I, and also far away
from the nucleus (Figure 9(c)) that is in stage II.
Regions of voids and of irregular and/or folded plates
are not uncommon in the central part of graphite
spheroids in cast iron, as shown in Figure 2(b). In view
of the findings presented in this communication, these
regions could be considered as exhibiting turbostratic
graphite. The elliptic Debye–Scherrer SAED and the
bent graphene layers in Figures 7(b) and (c) also indicate
a turbostratic structure.
This analysis leads to the conclusion that there is a
difference between the growth processes of SG formed
through liquid/solid transformation as in cast iron, and
graphite spheroids formed through solid/solid transfor-
mation (e.g., annealed carbon steel) or through gas/solid
transformation (e.g., pyrolysis). A schematic represen-
tation of the growth of a SG aggregate, as suggested by
this study, is presented in Figure 10. It is reasonable to
assume that most of the graphite that nucleates hetero-
geneously in cast iron starts its growth with the
formation of layers of turbostratic graphite. High
liquid/solid transformation temperature induces further
crystallization of the turbostratic graphite into graphene
layers that aggregate in the c-direction and expand in the
a-direction, developing into curved graphite platelets.
METALLURGICAL AND MATERIALS TRANSACTIONS B
Fig. 9—SAED patterns in three different regions of SG nucleated on a (Mg,Si,Al)N nitride: (a) crystalline region in the circle; (b) and (c)
turbostratic regions in the circle.
Fig. 10—Schematic representation of an SG grown in cast iron; the
amount of turbostratic graphite in regular SG is larger than it
appears in the figure.
These platelets continue to grow concentric to the
nucleus through a curved-circumferential mechanism as
long as the graphite is in contact with the liquid (stage I).
Once the graphite is encapsulated in the solid austenite
shell, growth through spiral dislocation or 2D poly-nu-
cleation continues to room temperature as cylindrical
columns or conical sectors. Occasionally, as shown in
METALLURGICAL AND MATERIALS TRANSACTIONS B
the figure, crystallization may start very close to the
nucleus (see Figure 9(a)) or it may advance to the point
that the curved platelets become part of the columns.
Also, turbostratic regions may exist in both stage I and
stage II. Examination of many SEM images of SG (e.g.,
Figures 2 and 4), reveals that voids and defects are an
often occurrence in both the curved platelets and
columnar region. This explains the high percentage of
turbostratic graphite in SG iron found by Ohbuchi
et al.[29]
By contrast, the graphite spheroid (~ 2 to 5 lm in
diameter) formed in annealed carbon steel is the product
of one stage crystallization initiated in many instances
on preexisting graphite, on foreign particles (e.g., AlN),
or on dissolving cementite particles[13,14] producing
cones or columns of graphene layers stacked in the
c-direction. In this case, as during graphite formation in
cast iron, the graphite core region shows turbostratic
regions structure while the outer layer has a strong
graphitic character.
ACKNOWLEDGMENTS
The authors would like to acknowledge Diputacion
Foral de Bizkaia for supporting this research.
VOLUME 54B, OCTOBER 2023—2289
 CONFLICT OF INTEREST
On behalf of all authors, the corresponding author
states that there is no conflict of interest.
DATA AVAILABILITY
None.
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